13C SPE MAS measurement of ligand concentration in compressible chromatographic beads

被引:3
作者
Elwinger, Fredrik [1 ,2 ]
Dvinskikh, Sergey V. [1 ]
Furo, Istvan [1 ]
机构
[1] KTH Royal Inst Technol, Div Appl Phys Chem, SE-10044 Stockholm, Sweden
[2] GE Healthcare Biosci AB, SE-75184 Uppsala, Sweden
基金
瑞典研究理事会;
关键词
NMR; C-13; solid-state NMR; quantitative NMR; agarose; pore; SOLID-STATE NMR; NUCLEAR-MAGNETIC-RESONANCE; ANGLE-SPINNING NMR; HYDROPHOBIC INTERACTION CHROMATOGRAPHY; SUPERCRITICAL CARBON-DIOXIDE; MODEL ORGANIC-COMPOUNDS; STATIONARY PHASES; QUANTITATIVE-DETERMINATION; CROSS-POLARIZATION; LIQUID-CHROMATOGRAPHY;
D O I
10.1002/mrc.4257
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
A method for measuring the ligand concentration in heterogeneous materials like chromatography media is described. In this method, C-13 single pulse excitation magic angle spinning NMR experiment with broadband H-1 decoupling is used to determine the peak integrals for a butyl ligand in the spectrum of a dried chromatography medium. Within a carefully controlled protocol, those integrals compared with that of the internal reference compound dimethyl sulfone provide the required volume concentration with an accuracy of ca 2%. The effects of temperature, degree of hydration, and other experimental parameters are discussed. Copyright (C) 2015 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.
引用
收藏
页码:572 / 577
页数:6
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